CN106517271A - Preparation method of magnesium-aluminum hydrotalcite nanosheet - Google Patents
Preparation method of magnesium-aluminum hydrotalcite nanosheet Download PDFInfo
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- CN106517271A CN106517271A CN201611042915.4A CN201611042915A CN106517271A CN 106517271 A CN106517271 A CN 106517271A CN 201611042915 A CN201611042915 A CN 201611042915A CN 106517271 A CN106517271 A CN 106517271A
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- preparation
- nanometer sheet
- magnalium hydrotalcite
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape
Abstract
The invention relates to the technical field of functional materials and particularly relates to a preparation method of a magnesium-aluminum hydrotalcite nanosheet. The preparation method comprises the following steps: (I) dissolving MgCl2 and AlCl3 in 25mL of deionized water to obtain a mixed salt solution A; (II) dissolving NH4HCO3 and CO(NH2)2 in 25mL of deionized water to obtain an alkaline solution B; (III) dissolving PEG in the solution A and stirring uniformly, adding the mixed alkaline solution B into the mixed salt solution A, and performing magnetic stirring; (IV) stirring uniformly, pouring 50mL of suspension into a reaction kettle lining, and performing a hydrothermal reaction in a dryer; (V) after the reaction, naturally cooling to room temperature, performing centrifugal washing with deionized water and alcohol respectively for 4 times, drying the product, taking out the product and grinding to obtain white powder; and (VI) putting a precursor MgAl-LDH product into a tubular furnace and heating, preserving heat in air for 4h, and cooling along with the furnace to obtain the magnesium-aluminum hydrotalcite nanosheet. In the invention, the prepared nanosheet has more complete and uniform crystal phase structure and better dispersity.
Description
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of preparation method of magnalium hydrotalcite nanometer sheet.
Background technology
Magnalium hydrotalcite is a kind of laminated type bimetal hydroxide compound, and M (II) and M (III) is respectively divalence and trivalent metal
Cation, An-For interlayer exchangeable anions, to maintain charge balance, holding structure is stable.Hydrotalcite after roasting takes off
Water becomes stratiform double oxide, can reuptake anion and recover its structure, with unique structure " memory effect ".LDH
With LDO because of its special interlayer structure, memory effect, with excellent ion exchange or absorption property, catalysis, photochemistry,
The fields such as biomedicine, electrochemistry, environmental protection have a wide range of applications.The performance of hydrotalcite with its constitute, microstructure, pattern and
Surface state is closely related.Various patterns, the hydrotalcite of composition include NiAl-LDH films, NiAl-LDH microballoons, MgAl-LDH
Nano particle, MgAl-LDH nanometer rods, MgAl-LDH nanometer sheets, flower-shaped MgAl-LDH nanostructureds, CoAl-LDH nanometer sheets,
NiFe-LDH nanometer sheets are widely studied.Because there are a large amount of non-bridge formation hydroxyls in hydrotalcite surface so that between adjacent particle easily
It is combined together by hydrogen bond action in dry run, causes the uneven dispersiveness of particle size just poor, thus improve its dispersion
Property be conducive to improve its performance.If the growth of control hydrotalcite nano piece forms it into cross-brace construction and is beneficial to its point
The improvement of scattered property, the research of current this respect are rarely reported.
The content of the invention
It is contemplated that proposing a kind of preparation method of magnalium hydrotalcite nanometer sheet.
Technical program of the present invention lies in：
The preparation method of magnalium hydrotalcite nanometer sheet, comprises the steps：
The first step, by MgCl2And AlCl3It is dissolved in 25mL deionized waters, is made into mixing salt solution A；
Second step, by NH4HCO3With CO (NH2)2 It is dissolved in 25mL deionized waters, proportionaling alkali-forming solution B；
PEG is dissolved in A solution, is stirred by the 3rd step, then mixed ammonium/alkali solutions B is added in mixing salt solution A, is entered
Row magnetic agitation；
4th step, after stirring pours 50mL suspensions in inner liner of reaction kettle into, carries out hydro-thermal reaction in an oven；
5th step, after reaction terminates, naturally cools to room temperature, deionized water and alcohol difference centrifuge washing 4 times, and product is done
It is dry, after taking out grinding, obtain white powder；
Presoma MgAl-LDH products are put into tube furnace and are heated up by the 6th step, are incubated along with the furnace cooling after 4h, system in atmosphere
Into magnalium hydrotalcite nanometer sheet.
Described MgCl2Concentration be 0.1 ~ 0.2mol, AlCl3Concentration be 0.05 ~ 0.1mol.
Described NH4The concentration of HCO is 0.2 ~ 0.3mol, CO (NH2)2Concentration be 0.2 ~ 0.3mol.
The time of the magnetic agitation in the 3rd described step is 30 ~ 45min.
The described temperature for carrying out hydro-thermal reaction in an oven is 130 ~ 150 DEG C, and the reaction time is 13 ~ 15h.
The temperature of described drying is 80 ~ 100 DEG C, and drying time is 6 ~ 7h.
Ramp to 500 DEG C of the heating rate of described tube furnace for 5 ~ 6 DEG C/min.
The method have technical effect that：
The present invention is controlled to the growth course of hydrotalcite using polyethylene glycol, has synthesized hexagonal flake using one step hydro thermal method
The Mg-Al type hydrotalcite nano pieces of pattern.Obtained Nano lamellite phase structure is more complete homogeneous, and dispersiveness is more preferably；It is corresponding to be obtained
Nanometer sheet absorption property significantly improve so as to wastewater treatment and reclaim field.
It is with a wide range of applications.
Specific embodiment
The preparation method of magnalium hydrotalcite nanometer sheet, comprises the steps：
Embodiment 1
The first step, by MgCl2And AlCl3It is dissolved in 25mL deionized waters, is made into mixing salt solution A；
Second step, by NH4HCO3With CO (NH2)2 It is dissolved in 25mL deionized waters, proportionaling alkali-forming solution B；
PEG is dissolved in A solution, is stirred by the 3rd step, then mixed ammonium/alkali solutions B is added in mixing salt solution A, is entered
Row magnetic agitation；
4th step, after stirring pours 50mL suspensions in inner liner of reaction kettle into, carries out hydro-thermal reaction in an oven；
5th step, after reaction terminates, naturally cools to room temperature, deionized water and alcohol difference centrifuge washing 4 times, and product is done
It is dry, after taking out grinding, obtain white powder；
Presoma MgAl-LDH products are put into tube furnace and are heated up by the 6th step, are incubated along with the furnace cooling after 4h, system in atmosphere
Into magnalium hydrotalcite nanometer sheet.
Wherein, MgCl2Concentration be 0.1mol, AlCl3Concentration be 0.05mol.Described NH4The concentration of HCO is
0.2mol, CO (NH2)2Concentration be 0.2mol.The time of the magnetic agitation in the 3rd described step is 30min.Described is drying
The temperature that hydro-thermal reaction is carried out in case is 130 DEG C, and the reaction time is 13h.The temperature of described drying is 80 DEG C, and drying time is
6h.Ramp to 500 DEG C of the heating rate of described tube furnace for 5 DEG C/min.
Embodiment 2
The first step, by MgCl2And AlCl3It is dissolved in 25mL deionized waters, is made into mixing salt solution A；
Second step, by NH4HCO3With CO (NH2)2 It is dissolved in 25mL deionized waters, proportionaling alkali-forming solution B；
PEG is dissolved in A solution, is stirred by the 3rd step, then mixed ammonium/alkali solutions B is added in mixing salt solution A, is entered
Row magnetic agitation；
4th step, after stirring pours 50mL suspensions in inner liner of reaction kettle into, carries out hydro-thermal reaction in an oven；
5th step, after reaction terminates, naturally cools to room temperature, deionized water and alcohol difference centrifuge washing 4 times, and product is done
It is dry, after taking out grinding, obtain white powder；
Presoma MgAl-LDH products are put into tube furnace and are heated up by the 6th step, are incubated along with the furnace cooling after 4h, system in atmosphere
Into magnalium hydrotalcite nanometer sheet.
Wherein, MgCl2Concentration be 0.2mol, AlCl3Concentration be 0.1mol.Described NH4The concentration of HCO is
0.3mol, CO (NH2)2Concentration be 0.3mol.The time of the magnetic agitation in the 3rd described step is 45min.Described is drying
The temperature that hydro-thermal reaction is carried out in case is 150 DEG C, and the reaction time is 15h.The temperature of described drying is 100 DEG C, drying time
For 7h.Ramp to 500 DEG C of the heating rate of described tube furnace for 6 DEG C/min.
Claims (7)
1. the preparation method of magnalium hydrotalcite nanometer sheet, it is characterised in that：Comprise the steps：
The first step, by MgCl2And AlCl3It is dissolved in 25mL deionized waters, is made into mixing salt solution A；
Second step, by NH4HCO3With CO (NH2)2 It is dissolved in 25mL deionized waters, proportionaling alkali-forming solution B；
PEG is dissolved in A solution, is stirred by the 3rd step, then mixed ammonium/alkali solutions B is added in mixing salt solution A, is entered
Row magnetic agitation；
4th step, after stirring pours 50mL suspensions in inner liner of reaction kettle into, carries out hydro-thermal reaction in an oven；
5th step, after reaction terminates, naturally cools to room temperature, deionized water and alcohol difference centrifuge washing 4 times, and product is done
It is dry, after taking out grinding, obtain white powder；
Presoma MgAl-LDH products are put into tube furnace and are heated up by the 6th step, are incubated along with the furnace cooling after 4h, system in atmosphere
Into magnalium hydrotalcite nanometer sheet.
2. the preparation method of magnalium hydrotalcite nanometer sheet according to claim 1, it is characterised in that：Described MgCl2It is dense
Spend for 0.1 ~ 0.2mol, AlCl3Concentration be 0.05 ~ 0.1mol.
3. the preparation method of magnalium hydrotalcite nanometer sheet according to claim 1, it is characterised in that：Described NH4HCO's
Concentration is 0.2 ~ 0.3mol, CO (NH2)2Concentration be 0.2 ~ 0.3mol.
4. the preparation method of magnalium hydrotalcite nanometer sheet according to claim 1, it is characterised in that：In the 3rd described step
Magnetic agitation time be 30 ~ 45min.
5. the preparation method of magnalium hydrotalcite nanometer sheet according to claim 1, it is characterised in that：It is described in an oven
The temperature for carrying out hydro-thermal reaction is 130 ~ 150 DEG C, and the reaction time is 13 ~ 15h.
6. the preparation method of magnalium hydrotalcite nanometer sheet according to claim 1, it is characterised in that：The temperature of described drying
Spend for 80 ~ 100 DEG C, drying time is 6 ~ 7h.
7. the preparation method of magnalium hydrotalcite nanometer sheet according to claim 1, it is characterised in that：Described tube furnace
Ramp to 500 DEG C of the heating rate for 5 ~ 6 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201611042915.4A CN106517271A (en) | 2016-11-24 | 2016-11-24 | Preparation method of magnesium-aluminum hydrotalcite nanosheet |
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| CN201611042915.4A CN106517271A (en) | 2016-11-24 | 2016-11-24 | Preparation method of magnesium-aluminum hydrotalcite nanosheet |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109453777A (en) * | 2018-11-26 | 2019-03-12 | 中国华能集团清洁能源技术研究院有限公司 | α-Fe is improved based on ternary layered double-metal hydroxide2O3The method of photoelectrocatalysis hydrogen production by water decomposition performance |
| CN110433764A (en) * | 2019-08-13 | 2019-11-12 | 浙江理工大学 | A kind of double-hydroxide preparation method for fluorine absorption |
| CN111204782A (en) * | 2020-01-19 | 2020-05-29 | 中国科学院宁波材料技术与工程研究所 | Nitrite intercalation hydrotalcite material, aqueous resin composite coating and preparation method thereof |
| CN116603498A (en) * | 2023-07-06 | 2023-08-18 | 南京工业大学 | Phosphate adsorbent, and preparation method and application thereof |
-
2016
- 2016-11-24 CN CN201611042915.4A patent/CN106517271A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109453777A (en) * | 2018-11-26 | 2019-03-12 | 中国华能集团清洁能源技术研究院有限公司 | α-Fe is improved based on ternary layered double-metal hydroxide2O3The method of photoelectrocatalysis hydrogen production by water decomposition performance |
| CN110433764A (en) * | 2019-08-13 | 2019-11-12 | 浙江理工大学 | A kind of double-hydroxide preparation method for fluorine absorption |
| CN111204782A (en) * | 2020-01-19 | 2020-05-29 | 中国科学院宁波材料技术与工程研究所 | Nitrite intercalation hydrotalcite material, aqueous resin composite coating and preparation method thereof |
| CN116603498A (en) * | 2023-07-06 | 2023-08-18 | 南京工业大学 | Phosphate adsorbent, and preparation method and application thereof |
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Application publication date: 20170322 |
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